Designation D803 − 15 Standard Test Methods for Testing Tall Oil1 This standard is issued under the fixed designation D803; the number immediately following the designation indicates the year of origi[.]
Designation: D803 − 15 Standard Test Methods for Testing Tall Oil1 This standard is issued under the fixed designation D803; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision A number in parentheses indicates the year of last reapproval A superscript epsilon (´) indicates an editorial change since the last revision or reapproval Referenced Documents Scope 2.1 ASTM Standards:2 D92 Test Method for Flash and Fire Points by Cleveland Open Cup Tester D93 Test Methods for Flash Point by Pensky-Martens Closed Cup Tester D269 Test Method for Insoluble Matter in Rosin and Rosin Derivatives D464 Test Methods for Saponification Number of Naval Store Products Including Tall Oil and Other Related Products D465 Test Methods for Acid Number of Naval Stores Products Including Tall Oil and Other Related Products D890 Test Method for Water in Liquid Pine Chemicals D1065 Test Method for Unsaponifiable Matter in Naval Stores, Including Rosin, Tall Oil, and Related Products D1240 Test Methods for Rosin Acids Content of Pine Chemicals, Including Rosin, Tall Oil, and Related Products D1466 Test Method for Sampling Liquid Oils and Fatty Acids Commonly Used in Paints, Varnishes, and Related Materials (Withdrawn 2003)3 D1544 Test Method for Color of Transparent Liquids (Gardner Color Scale) D1545 Test Method for Viscosity of Transparent Liquids by Bubble Time Method D1585 Test Methods for Fatty Acids Content of Naval Stores, Including Rosin, Tall Oil, and Related Products D2196 Test Methods for Rheological Properties of NonNewtonian Materials by Rotational Viscometer D3278 Test Methods for Flash Point of Liquids by Small Scale Closed-Cup Apparatus D5974 Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography D6166 Test Method for Color of Pine Chemicals and Related Products (Instrumental Determination of Gardner Color) 1.1 These test methods cover the test procedures to be applied to whole tall oils or refined tall oils Previous editions of these test methods have described test procedures that are used to test tall oil fatty acid, rosin, and other tall oil-derived products as well as test crude and refined tall oil Consequently, these test methods are widely cited in reference books and industry literature for the testing of tall oil-derived products 1.1.1 In this current revision, procedural details of some of the often-cited test methods have been removed and the test methods consolidated with other existing test methods In such cases the consolidated methods, applicable to all tall oilderived products 1.2 The procedures appear in the following order: Physical Tests Viscosity: Rotational Viscometer Method (Preferred Method) Bubble Time Method Flash Point Color Moisture: Insoluble Matter Ash Chemical Analysis Acid Number Saponification Number Rosin Acids Unsaponifiable Matter Fatty Acids Sections 10 11 12 13 16 17 18 19 20 1.3 The values stated in inch-pound units are to be regarded as standard The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of Subcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins Current edition approved July 1, 2015 Published July 2015 Originally approved in 1944 Last previous edition approved in 2012 as D803 – 12 DOI: 10.1520/ D0803-15 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org For Annual Book of ASTM Standards volume information, refer to the standard’s Document Summary page on the ASTM website The last approved version of this historical standard is referenced on www.astm.org Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959 United States D803 − 15 VISCOSITY BY THE ROTATIONAL VISCOMETER METHOD (Preferred Method) E300 Practice for Sampling Industrial Chemicals Significance and Use 3.1 Tall oil, both crude and refined, is an important byproduct of the alkaline (kraft) pulping of pine wood It consists primarily of fatty acids, resin acids, and neutral materials; the levels of these various components depend on factors such as the species of pine tree, geographic location, climate, etc 3.1.1 Tall oil is used primarily as a commercial source of fatty acids and rosin, and, therefore, reliable methods for the analysis of these components is necessary Procedure 7.1 Determine the viscosity in centipoise in accordance with Test Methods D2196 The testing temperature shall be 210°F (99°C) unless a lower temperature is specified VISCOSITY BY THE BUBBLE TIME METHOD (Alternative Method) Procedure Purity of Reagents 8.1 Determine the viscosity in accordance with Test Method D1545 The testing temperature shall be 210°F (99°C) unless a lower temperature is specified 4.1 Reagent grade chemicals shall be used in all tests Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination FLASH POINT Procedure 9.1 Determine the flash point in accordance with any referenced method (see Test Methods D92, D93, and D3278) 4.2 Unless otherwise indicated, references to water shall be understood to mean distilled water or deionized water COLOR 10 Procedure Sampling 10.1 Determine the color in accordance with Test Methods D1544 or D6166 5.1 As with many industrial chemicals, the procedure for obtaining a representative sample of tall oil depends on the container to be sampled and the uniformity of the material to be sampled No specific standard procedure for sampling tall oil has been developed but Test Method D1466 and Practice E300 describe applicable methods when the tall oil contains no separated solids or separated water If rosin has separated, the rosin can be redissolved by heating and agitating the material to be sampled until it is homogeneous If separated water is present, special procedures should be followed to ensure that a representative sample be obtained The selection of an appropriate procedure will depend on the water content and the type of container being sampled MOISTURE CONTENT 11 Procedure 11.1 Determine the moisture content in accordance with the methods described in Test Method D890 The Karl Fischer method is the preferred method INSOLUBLE MATTER 12 Procedure 12.1 Determine the insoluble matter in accordance with Test Method D269 Conditioning 6.1 Heat the entire sample in a closed container fitted with a capillary vent or its equivalent Some kind of agitation, even if done occasionally by hand, saves much time Heat in a forced-air oven in order to dissolve any crystalline material A temperature of 100°C is usually sufficient to dissolve crystals present in crude tall oil, but a temperature as high as 160°C may be required to remove rosin crystals from distilled tall oil Withdraw the specimens only when all crystalline matter has dissolved and when the entire sample becomes a homogeneous fluid after thorough stirring ASH 13 Apparatus 13.1 Platinum Dish—A platinum dish of 50 to 100-mL capacity NOTE 1—A porcelain or silica dish may be used in place of platinum, if the ash is not to be analyzed 14 Procedure 14.1 Heat the platinum dish to redness and, after cooling in a desiccator, weigh to the nearest 0.0001 g Place an approximately 20-g sample of tall oil in the dish and weigh to the nearest 0.1 g (Note 2) Heat the dish gently by means of a bunsen burner until the oil can be ignited at the surface (Note 3) Remove the burner and allow the oil to burn completely Burn all free carbon on the sides of the dish and heat the Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S Pharmacopeial Convention, Inc (USPC), Rockville, MD D803 − 15 residue with a strong flame, or in a muffle furnace, until all carbonaceous matter disappears After cooling in a desiccator weigh the dish to the nearest 0.0001 g Repeat the heating until a constant weight is obtained 18 Rosin Acid Content NOTE 2—This size is suitable for ash contents in the range from 0.02 to 0.2 %, but in the case of lower or higher ash contents, a larger or smaller sample may be used In such cases the result shall be specified or reported as follows: “Ash ( g sample) percent.” NOTE 3—To avoid foaming and loss of sample in the case of samples containing moisture, it is advisable to add to mL of absolute alcohol before heating 19 Unsaponifiable Matter 18.1 Determine the rosin acid content in accordance with Test Methods D1240 19.1 Determine the unsaponifiable matter in accordance with Test Method D1065 20 Fatty Acid Content 20.1 Determine the fatty acid content in accordance with Test Methods D1585 15 Calculation 15.1 Calculate the percentage of ash as follows: Ash % ~ R/W ! 100 21 Gas Chromatographic Analysis (1) 21.1 Analyze for rosin acids and fatty acids in accordance with Test Methods D5974 where: R = residue, g, and W = sample, dry basis, g 22 Precision and Bias (General Statement) 15.2 Report the percentage of ash to the third decimal place 22.1 Where the test method listed in this standard references another ASTM method, that method should be studied to determine the precision and bias Other methods listed are well established, and determination of precision and bias is not practical CHEMICAL ANALYSIS 16 Acid Number 16.1 Determine the acid number in accordance with Test Methods D465 23 Keywords 17 Saponification Number 17.1 Determine the saponification number in accordance with Test Methods D464 23.1 acid number; fatty acids; rosin acids; saponification number; tall oil ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility This standard is 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